Hydrothermal Syntheses and Characterizations of Vanadium Phosphates with Extra-large 16-Ring Channels†

doi:10.7503/cjcu20140725

Abstract

Abstract:

Using n-butylamine, n-propylamine and piperidine as templates or structure directing agents(SDAs), three new open-framework vanadium phosphates VPO-n(n=1, 2, 3) were hydrothermally synthesized. These compounds were characterized by single-crystal and powder X-ray diffractions, ICP, elementary analysis, TGA, SEM and XPS analyses. VPO-1 crystallizes in the cubic system, space group Im3m, with a=b=c=2.6586(3) nm, α=β=γ=90°, V=18.791(4) nm³. The structure of VPO-1 has 3D intersecting 8-ring and extra-large 16-ring channels, as well as large cavities with 32-ring windows. VPO-n(n=1, 2, 3) are iso-structures, which are analogous to [HN(CH₂CH₂)₃NH]K_1.35[V₅O₉(PO₄)₂]·H₂O synthesized by triethylenediamine(DABCO) as template. Structure comparison of these compounds indicates that the organic templates not only influence the symmetry and cell parameters of the crystal structure, but also can control the opening sizes and shapes of the channels and the cages in the resulting structures.

Key words: Hydrothermal synthesis, Vanadium phosphate, Extra-large pore, Organic template

CLC Number:

O611.4

TrendMD:

LI Li, YAN Yan, WANG Daming, ZHENG Dafang, LI Jiyang. Hydrothermal Syntheses and Characterizations of Vanadium Phosphates with Extra-large 16-Ring Channels^†[J]. Chem. J. Chinese Universities, 2014, 35(11): 2285.

Figures/Tables 7

Fig.1 Simulated XRD pattern of VPO-DABCO(a) and experimental XRD patterns of VPO-1(b), VPO-2(c) and VPO-3(d)

Fig.2 Asymmetric unit of VPO-1 without n-butylamine and H2O molecules

Fig.3 Curved pentameric {V5O9(PO4)2} unit(A), the open-framework structure viewed along the [100] direction showing the 8-ring and the extra-large 16-ring channels(B) and the large cavity with 32-ring window(C)

Fig.4 TG curves of VPO-1(a), VPO-2(b) and VPO-3(c)

Fig.5 XPS spectra of VPO-1(A), VPO-2(B) and VPO-3(C)

Fig.6 SEM images of VPO-1(A), VPO-2(B) and VPO-3(C)

Fig.7 Rectangular 16-ring window(left) and large cavity(right) in VPO-1(A) and VPO-DABCO(B)

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